CN106283610A - A kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method - Google Patents
A kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method Download PDFInfo
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Abstract
The invention discloses a kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method, belong to conducing composite material preparation field.The method is at the three-layer laminated Graphene of flexible parent metal surface-assembled, by the layer structure inductive formation large-area nanometer wire polypyrrole of Graphene.The features such as it is high that three-layer laminated Graphene inductive formation polypyrrole nano line flexible conductive composite material prepared by the method has specific surface area, conducts electricity very well, and reproduction performance is good, simple for process.Wearable electronic product, electrochemical transistor electrode material, electrode material for super capacitor, microbiological fuel cell, the field such as sensor can be widely used in.
Description
Technical field
The invention discloses a kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method, belong to and lead
Composite preparing technical field.
Background technology
Fiber, the flexible parent metal such as fabric is due to frivolous, and soft stretch-proof and loose structure can load a large amount of active substance,
It it is considered as the preferable base material of preparation wearable electronic.A lot of researchers are the most successfully by CNT, Graphene etc.
The electrode materials such as material with carbon element is compound with fiber or fabric is formed with dynamo-electric chemical transistor, ultracapacitor.
Graphene be a kind of be the flat film of honeycomb lattice with the hexangle type that sp2 hybrid orbital forms by carbon atom, only
There is the Two-dimensional Carbon material of a carbon atom thickness.From 2004, Univ Manchester UK physicist An Deliegaimu and
Graphene is isolated in the success of Constantine's Nuo Woxiao love from graphite, because of its mechanical mechanics property, electric conductivity excellence, high
Specific surface area and room temperature electron mobility and electrochemical stability are good, and charge-transfer resistance is little, and electron transfer rate is fast, electrification
Learn the excellent properties such as window width to be widely studied.
Polypyrrole is a kind of important conducting polymer, and owing to raw material is easy to get, synthesis is simple, and antioxygenic property is good, stable,
Easily film forming, after doping, the more high series of advantages of conductivity is by the extensive concern of researcher.The invention discloses one
Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation method, utilizes the three-layer laminated knot that Graphene is special
Structure, at flexible parent metal Surface Creation polypyrrole nano line shape conductive material.
Summary of the invention
A kind of Graphene inductive formation polypyrrole nano line conducing composite material system of offer is provided
Preparation Method, to achieve these goals, the technical solution used in the present invention is:
A kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method, improves including using
Hammers method prepares three-layer laminated graphene oxide solution, and described preparation method sequentially includes the following steps:
A. prepared by flexible parent metal/three-layer laminated Graphene
Fully being soaked in flexible parent metal to use improves in three-layer laminated graphene oxide solution prepared by Hammers method,
Three-layer laminated graphene oxide concentration is 0.2%-5%, and flexible parent metal and three-layer laminated graphene oxide soak time are 1-
10h, the flexible parent metal after soaking hangs in reactor, and adding volume is the reducing agent of 5-30ml, seals, in fume hood
Heating in water bath, bath temperature is 60-100 DEG C, and the thermal response time is 1-4h, and oxygen-containing group is removed in fully reduction, obtains three-layer laminated
Graphene/flexible parent metal.
B. the preparation of flexible parent metal/three-layer laminated Graphene/polypyrrole nano line conducing composite material
Three-layer laminated Graphene/the flexible parent metal described step a obtained mixes on shaking table with pyrroles and surfactant
Closing uniformly, wherein pyrroles and surfactant qualities ratio is for 1:0.5-2, is together placed in agitator, and mixing speed is 600r/
Min, is slowly added to the mixed solution of oxidant and adulterant under condition of ice bath, and wherein oxidant with the mol ratio of adulterant is
1:0.2-2；Reaction 1-5h, obtains three-layer laminated Graphene/polypyrrole nano line flexible conductive composite material.
Described flexible parent metal be in line base material or cloth base material any one.
Described line base material is the one in nylon 6 doubling or polyethylene strand or cotton thread, and line length substrate is 20-
100cm。
Described cloth base material be in carbon cloth or cotton or woven dacron or nylon cloth or polyethylene cloth any one；Cloth base material chi
Very little is 2 × 2-5 × 5cm2。
Described reducing agent is the mixture of ammonia or hydrazine hydrate or hydroiodic acid and glacial acetic acid, and wherein the volume fraction of ammonia is
50%, the volume fraction of hydrazine hydrate is 85%, and between hydroiodic acid and glacial acetic acid, volume ratio is 1-10:10-1.
Described surfactant is dodecyl sodium sulfate or dodecylbenzene sodium sulfonate or anthraquinone-2-sodium or gathers
In vinylpyrrolidone any one；Described surfactant water concentration is 5-30mg/mL.
Described oxidant is to appoint in Fe(NO3)39H2O or iron chloride or Ammonium persulfate. or potassium peroxydisulfate or manganese dioxide
Meaning one.
Described adulterant is any one in two hydration 5-sulphosalicylic acids or sulphuric acid or hydrochloric acid or phosphoric acid or nitric acid.
Technical scheme scheme compared to existing technology has the advantage that
The preparation method of a kind of Graphene inductive formation polypyrrole nano line conducing composite material of the present invention, is with flexibility
Base material is template, and a compound layer graphene thin film on base material, the three-layer laminated structure of Graphene can be received by inductive formation polypyrrole
Rice noodle.The three-layer laminated Graphene inductive formation polypyrrole nano line flexible conductive composite material prepared by the method has ratio
The features such as surface area is high, conducts electricity very well, and reproduction performance is good, simple for process.Electrochemical transistor can be widely used in
Electrode material, electrode material for super capacitor, microbiological fuel cell, the field such as sensor.
Accompanying drawing explanation
Fig. 1 is the SEM comparison figure of nylon 6 doubling in embodiment 1 and nylon 6 doublings/Graphene/polypyrrole.
Fig. 2 is the SEM comparison figure of the carbon cloth in embodiment 4 and carbon cloth/Graphene/polypyrrole.
Fig. 3 is the SEM comparison figure of the cotton in embodiment 8 and cotton/Graphene/polypyrrole.
Detailed description of the invention
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is described in further detail.
A kind of Graphene inductive formation polypyrrole nano line conducing composite material preparation method, this preparation method is based on improvement
Hammers method is carried out on the basis of preparing graphene oxide solution.Refering to document (J.Mater.Chem.22,2012,1396-
1402)。
Described preparation method sequentially includes the following steps:
A. prepared by flexible parent metal/three-layer laminated Graphene
Fully being soaked in flexible parent metal to use improves in three-layer laminated graphene oxide solution prepared by Hammers method,
Three-layer laminated graphene oxide concentration is 0.2%-5%, and flexible parent metal and three-layer laminated graphene oxide soak time are 1-
10h, the flexible parent metal after soaking hangs in reactor, and adding volume is the reducing agent of 5-30ml, seals, water in fume hood
Bath heating, bath temperature is 60-100 DEG C, and the thermal response time is 1-4h, and oxygen-containing group is removed in fully reduction, obtains three-layer laminated stone
Ink alkene/flexible parent metal.
Described flexible parent metal be in line base material or cloth base material any one.
Described line base material is the one in nylon 6 doubling or polyethylene strand or cotton thread, and line length substrate is 20-
100cm。
Described cloth base material be in carbon cloth or cotton or woven dacron or nylon cloth or polyethylene cloth any one；Cloth base material chi
Very little is 2 × 2-5 × 5cm2。
Described reducing agent is the mixture of ammonia or hydrazine hydrate or hydroiodic acid and glacial acetic acid, and wherein the volume fraction of ammonia is
50%, the volume fraction of hydrazine hydrate is 85%, and between hydroiodic acid and glacial acetic acid, volume ratio is 1-10:10-1.
B. the preparation of flexible parent metal/three-layer laminated Graphene/polypyrrole nano line conducing composite material
Three-layer laminated Graphene/the flexible parent metal described step a obtained mixes on shaking table with pyrroles and surfactant
Closing uniformly, wherein pyrroles and surfactant qualities ratio is for 1:0.5-2, is together placed in agitator, and mixing speed is 600r/
Min, is slowly added to the mixed solution of oxidant and adulterant under condition of ice bath, and wherein oxidant with the mol ratio of adulterant is
1:0.2-2；Reaction 1-5h, obtains three-layer laminated Graphene/polypyrrole nano line flexible conductive composite material.
Described surfactant is dodecyl sodium sulfate or dodecylbenzene sodium sulfonate or anthraquinone-2-sodium or gathers
In vinylpyrrolidone any one；Described surfactant water concentration is 5-30mg/mL.
Described oxidant is to appoint in Fe(NO3)39H2O or iron chloride or Ammonium persulfate. or potassium peroxydisulfate or manganese dioxide
Meaning one.
Described adulterant is any one in two hydration 5-sulphosalicylic acids or sulphuric acid or hydrochloric acid or phosphoric acid or nitric acid.
Specific embodiment
Embodiment 1
The present embodiment is with nylon 6 doubling base material as template, and in nylon 6 doubling, compound one layer of three-layer laminated Graphene is thin
Film, generates nylon 6/ Graphene/polypyrrole nano line flexible conductive composite material under three-layer laminated Graphene inducing action.Institute
State preparation method to follow the steps below:
A. prepared by nylon 6 doubling base material/three-layer laminated Graphene
It is 0.2% three-layer laminated graphene oxide that 20cm nylon 6 doubling base material is soaked in concentration, and soak time is 1h,
Obtain nylon 6 doubling base material/graphene oxide.
Hanging in reactor by nylon 6/ graphene oxide sample, add 5mL ammonia, seal, in fume hood, water-bath adds
Heat, bath temperature is 60 DEG C, and the response time is 1h, obtains nylon 6 doubling base material/Graphene.
B. the preparation of nylon 6 doubling base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
127.105g Fe(NO3)39H2O and 6.03g nitric acid are dissolved in 500mL deionized water to uniform mixed liquor, take
This iron salt mixed liquor of 100mL, puts into refrigerator lower floor freezing 5min.
20cm nylon 6/ Graphene in above-mentioned steps a being placed in 0.25g pyrroles with 100mL concentration is the 12 of 5mg/mL
In the mixed liquor of alkyl sulfonic acid sodium water solution, shaking table mixes 2min, takes out, take out after putting into refrigerator lower floor freezing 5min,
Together being placed in agitator, mixing speed is to be slowly added dropwise 100mL above-mentioned iron salt mixed liquor under 600r/min, condition of ice bath.Instead
Take out after answering 1h and obtain nylon 6 doubling base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material.
Described nylon 6 doubling base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material SEM schemes such as accompanying drawing
1。
Embodiment 2
The present embodiment is with polyethylene strand base material as template, and on polyethylene strand, compound one layer of three-layer laminated Graphene is thin
Film, generates polyethylene strand/Graphene/polypyrrole nano line compliant conductive composite wood under three-layer laminated Graphene inducing action
Material.Described preparation method follows the steps below:
A. prepared by polyethylene strand base material/three-layer laminated Graphene
60cm polyethylene strand base material is soaked in the three-layer laminated graphene oxide that concentration is 0.5%, and soak time is
2h, obtains polyethylene/graphene oxide.
Hanging in reactor by polyethylene strand base material/graphene oxide sample, adding 10mL volume fraction is 50%
Hydrazine hydrate, seal, heating in water bath in fume hood, bath temperature is 70 DEG C, and the response time is 1.5h, obtains polyethylene strand base
Material/Graphene.
B. the preparation of polyethylene strand base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
127.105g Fe(NO3)39H2O and 50.842g 5-sulphosalicylic acid are dissolved in 500mL deionized water obtain uniformly
Mixed liquor, takes this iron salt mixed liquor of 100mL, puts into refrigerator lower floor freezing 5min.
60cm polyethylene strand base material/Graphene in above-mentioned steps b being placed in 0.4g pyrroles with 100mL concentration is 8mg/
In the mixed liquor of the sodium dodecyl benzene sulfonate aqueous solution of mL, shaking table mixes 2min, takes out, put into refrigerator lower floor freezing
Taking out after 5min, be together placed in agitator, mixing speed is to be slowly added dropwise the above-mentioned ferrum of 100mL under 600r/min, condition of ice bath
Salt mixed liquor.Take out after reaction 1.5h that to obtain polyethylene strand base material/three-layer laminated Graphene/polypyrrole nano line conduction compound
Material.
Embodiment 3
The present embodiment is with cotton thread doubling base material as template, and compound one layer of three-layer laminated graphene film on cotton thread, three
Cotton thread/Graphene/polypyrrole nano line flexible conductive composite material is generated under dimension lamellar graphite alkene inducing action.Described preparation side
Method follows the steps below:
A. prepared by cotton thread base material/three-layer laminated Graphene
100cm cotton thread base material is soaked in the three-layer laminated graphene oxide that concentration is 1%, and soak time is 3h, obtains
Cotton thread/graphene oxide.
Hanging in reactor by cotton thread/graphene oxide sample, adding 15mL volume fraction is the hydrazine hydrate of 85%, close
Envelope, heating in water bath in fume hood, bath temperature is 80 DEG C, and the response time is 4h, obtains cotton thread/Graphene.
B. the preparation of cotton thread base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
81.102g iron chloride and 10.938g hydrochloric acid are dissolved in 500mL deionized water to uniform mixed liquor, taking 100mL should
Iron salt mixed liquor, puts into refrigerator lower floor freezing 5min.
100cm cotton thread/Graphene in above-mentioned steps b being placed in 1.2g pyrroles with 100mL concentration is the anthracene of 10mg/mL
In the mixed liquor of quinone-2-sodium sulfonate aqueous solution, shaking table mixes 2min, takes out, take out after putting into refrigerator lower floor freezing 5min,
Together being placed in agitator, mixing speed is to be slowly added dropwise 100mL above-mentioned iron salt mixed liquor under 600r/min, condition of ice bath.Instead
Take out after answering 2h and obtain cotton thread base material/Graphene/polypyrrole nano line conducing composite material.
Embodiment 4
The present embodiment is with carbon cloth base material as template, and compound one layer of three-layer laminated graphene film on carbon cloth, in three-dimension layer
Carbon cloth base material/Graphene/polypyrrole nano line flexible conductive composite material is generated under shape Graphene inducing action.Described preparation side
Method follows the steps below:
A. prepared by carbon cloth base material/three-layer laminated Graphene
By 2 × 2cm2Carbon cloth base material is soaked in the three-layer laminated graphene oxide that concentration is 2%, and soak time is 5h,
To carbon cloth/graphene oxide.
Carbon cloth/graphene oxide sample is hung in reactor, adds 20mL hydroiodic acid and glacial acetic acid mixed liquor, wherein
Hydroiodic acid and glacial acetic acid volume ratio are 1:10, seal, heating in water bath in fume hood, and bath temperature is 80 DEG C, and the response time is 2h,
Obtain carbon cloth/Graphene.
B. the preparation of carbon cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
81.102g iron chloride is dissolved in 127.105g 5-sulphosalicylic acid 500mL deionized water to uniformly mixing
Liquid, takes this iron salt mixed liquor of 100mL, puts into refrigerator lower floor freezing 5min.
By the 2*2cm in above-mentioned steps a2It is 15mg/mL that carbon cloth/Graphene base material is placed in 1.5g pyrroles with 100mL concentration
Aqueous povidone solution mixed liquor in, on shaking table mix 2min, take out, after putting into refrigerator lower floor freezing 5min
Taking out, be together placed in agitator, mixing speed is to be slowly added dropwise the mixing of 100mL above-mentioned iron salt under 600r/min, condition of ice bath
Liquid.Take out after reaction 2.5h and obtain carbon cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material.
Described carbon cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material SEM schemes such as accompanying drawing 2.
Embodiment 5
The present embodiment, with woven dacron base material as template, is combined one layer of three-layer laminated graphene film on woven dacron base material,
Woven dacron base material/Graphene/polypyrrole nano line flexible conductive composite material is generated under three-layer laminated Graphene inducing action.
Described preparation method follows the steps below:
A. prepared by woven dacron base material/three-layer laminated Graphene
By 3 × 3cm2Woven dacron base material is soaked in the three-layer laminated graphene oxide that concentration is 3%, and soak time is 6h,
Obtain woven dacron/graphene oxide.
Woven dacron base material/graphene oxide sample is hung in reactor, adds 25mL hydroiodic acid and mix with glacial acetic acid
Liquid, wherein hydroiodic acid and glacial acetic acid volume ratio are 3:8, seal, and heating in water bath in fume hood, bath temperature is 80 DEG C, during reaction
Between be 2.5h, obtain woven dacron/Graphene.
B. the preparation of woven dacron base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
114.095g Ammonium persulfate. and 68.655g sulphuric acid are dissolved in 500mL deionized water to uniform mixed liquor, take
This iron salt mixed liquor of 100mL, puts into refrigerator lower floor freezing 5min.
By the 3*3cm in above-mentioned steps a2Woven dacron base material/Graphene base material is placed in 2.8g pyrroles and with 100mL concentration is
In the mixed liquor of the sodium dodecyl sulfate aqueous solution of 20mg/mL, shaking table mixes 2min, takes out, put into refrigerator lower floor cold
Freezing and take out after 5min, be together placed in agitator, mixing speed is that to be slowly added dropwise 100mL under 600r/min, condition of ice bath above-mentioned
Iron salt mixed liquor.Take out after reaction 3h and obtain woven dacron base material/three-layer laminated Graphene/polypyrrole nano line conduction composite wood
Material.
Embodiment 6
The present embodiment is with nylon cloth base material as template, and compound one layer of three-layer laminated graphene film on nylon cloth, three
Nylon cloth/Graphene/polypyrrole nano line flexible conductive composite material is generated under dimension lamellar graphite alkene inducing action.Described preparation
Method follows the steps below:
A. prepared by nylon cloth base material/three-layer laminated Graphene
By 3.5 × 3.5cm2Nylon cloth base material is soaked in the three-layer laminated graphene oxide that concentration is 3.5%, soak time
For 7h, obtain nylon cloth/graphene oxide.
Nylon cloth/graphene oxide sample is hung in reactor, adds 30mL hydroiodic acid and glacial acetic acid mixed liquor, its
Middle hydroiodic acid and glacial acetic acid volume ratio are 5:6, seal, heating in water bath in fume hood, and bath temperature is 90 DEG C, and the response time is
3h, obtains nylon cloth/Graphene.
B. the preparation of nylon cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
114.095g Ammonium persulfate. and 50.408g nitric acid are dissolved in 500mL deionized water to uniform mixed liquor, take
This iron salt mixed liquor of 100mL, puts into refrigerator lower floor freezing 5min.
By 3.5 × 3.5cm in above-mentioned steps a2It is 25mg/mL that nylon cloth/Graphene is placed in 4g pyrroles with 100mL concentration
Sodium dodecyl benzene sulfonate aqueous solution mixed liquor in, on shaking table mix 2min, take out, put into refrigerator lower floor freezing 5min
Rear taking-up, is together placed in agitator, and mixing speed is to be slowly added dropwise the above-mentioned iron salt of 100mL under 600r/min, condition of ice bath to mix
Close liquid.Take out after reaction 3.5h and obtain nylon cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material.
Embodiment 7
The present embodiment, with polyethylene cloth base material as template, is combined one layer of three-layer laminated graphene film on polyethylene cloth,
Polyethylene cloth base material/Graphene/polypyrrole nano line compliant conductive composite wood is generated under three-layer laminated Graphene inducing action
Material.Described preparation method follows the steps below:
A. prepared by polyethylene cloth base material/three-layer laminated Graphene
By 4 × 4cm2Polyethylene cloth base material is soaked in the three-layer laminated graphene oxide that concentration is 4%, and soak time is
8h, obtains polyethylene cloth/graphene oxide.
Polyethylene cloth/graphene oxide sample is hung in reactor, adds 30mL hydroiodic acid and glacial acetic acid mixed liquor,
Wherein hydroiodic acid and glacial acetic acid volume ratio are 7:4, seal, and heating in water bath in fume hood, bath temperature is 100 DEG C, the response time
For 4h, obtain polyethylene cloth/Graphene.
B. the preparation of polyethylene cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
135.16g potassium peroxydisulfate and 88.270g sulphuric acid are dissolved in 500mL deionized water to uniform mixed liquor, take 100mL
This iron salt mixed liquor, puts into refrigerator lower floor freezing 5min.
By 4 × 4cm in above-mentioned steps a2It is 28mg/ that polyethylene cloth/Graphene is placed in 5.04g pyrroles with 100mL concentration
In the mixed liquor of the anthraquinone-2-sulfonic acid sodium water solution of mL, shaking table mixes 2min, takes out, put into refrigerator lower floor freezing 5min
Rear taking-up, is together placed in agitator, and mixing speed is to be slowly added dropwise the above-mentioned iron salt of 100mL under 600r/min, condition of ice bath to mix
Close liquid.Take out after reaction 4h and obtain polyethylene cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material.
Embodiment 8
The present embodiment is with cotton base material as template, and compound one layer of three-layer laminated graphene film on cotton base material, three
Cotton base material/Graphene/polypyrrole nano line flexible conductive composite material is generated under dimension lamellar graphite alkene inducing action.Described system
Preparation Method follows the steps below:
A. prepared by cotton base material/three-layer laminated Graphene
By 5 × 5cm2Cotton base material is soaked in the three-layer laminated graphene oxide in above-mentioned steps a that concentration is 5%, leaching
The bubble time is 9h, obtains cotton/graphene oxide.
Cotton/graphene oxide sample is hung in reactor, adds 30mL hydroiodic acid and glacial acetic acid mixed liquor, wherein
Hydroiodic acid and glacial acetic acid volume ratio are 10:1, seal, heating in water bath in fume hood, and bath temperature is 100 DEG C, and the response time is
4h, obtains cotton/Graphene.
B. the preparation of cotton base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
43.47g manganese dioxide and 98g sulphuric acid are dissolved in 500mL deionized water to uniform mixed liquor, take this ferrum of 100mL
Salt mixed liquor, puts into refrigerator lower floor freezing 5min.
By 5 × 5cm in above-mentioned steps a2It is 30mg/mL's that cotton base material/Graphene is placed in 6g pyrroles with 100mL concentration
In the mixed liquor of aqueous povidone solution, shaking table mixes 2min, takes out, take after putting into refrigerator lower floor freezing 5min
Going out, be together placed in agitator, mixing speed is to be slowly added dropwise 100mL above-mentioned iron salt mixed liquor under 600r/min, condition of ice bath.
Take out after reaction 5h and obtain cotton base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material.
Described cotton base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material SEM schemes such as accompanying drawing 3.
Embodiment 9
The present embodiment is with cotton base material as template, and compound one layer of three-layer laminated graphene film on cotton, in three-dimension layer
Cotton base material/Graphene/polypyrrole nano line flexible conductive composite material is generated under shape Graphene inducing action.Described preparation side
Method follows the steps below:
A. prepared by cotton base material/three-layer laminated Graphene
By 4.5 × 4.5cm2Cotton base material is soaked in the three-layer laminated graphite oxide in above-mentioned steps a that concentration is 4%
Alkene, soak time is 9h, obtains cotton/graphene oxide.
Cotton base material/graphene oxide sample is hung in reactor, adds 25mL hydroiodic acid and glacial acetic acid mixed liquor,
Wherein hydroiodic acid and glacial acetic acid volume ratio are 9:2, seal, and heating in water bath in fume hood, bath temperature is 100 DEG C, the response time
For 4h, obtain cotton/Graphene.
B. the preparation of cotton base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
43.47g manganese dioxide and 20g hydrochloric acid are dissolved in 500mL deionized water to uniform mixed liquor, take this ferrum of 100mL
Salt mixed liquor, puts into refrigerator lower floor freezing 5min.
By 4.5 × 4.5cm in above-mentioned steps a2Cotton base material/Graphene is placed in 5.5g pyrroles and with 100mL concentration is
In the mixed liquor of the aqueous povidone solution of 28mg/mL, shaking table mixes 2min, takes out, put into refrigerator lower floor cold
Freezing and take out after 5min, be together placed in agitator, mixing speed is that to be slowly added dropwise 100mL under 600r/min, condition of ice bath above-mentioned
Iron salt mixed liquor.Take out after reaction 5h and obtain cotton base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material.
Embodiment 10
The present embodiment, with polyethylene cloth base material as template, is combined one layer of three-layer laminated graphene film on polyethylene cloth,
Polyethylene cloth base material/Graphene/polypyrrole nano line compliant conductive composite wood is generated under three-layer laminated Graphene inducing action
Material.Described preparation method follows the steps below:
A. prepared by polyethylene cloth base material/three-layer laminated Graphene
By 2.5 × 2.5cm2Polyethylene cloth base material is soaked in the three-layer laminated graphene oxide that concentration is 3%, soak time
For 8h, obtain polyethylene/graphene oxide.
Polyethylene cloth base material/graphene oxide sample is hung in reactor, adds 20mL hydroiodic acid and mix with glacial acetic acid
Closing liquid, wherein hydroiodic acid and glacial acetic acid volume ratio are 5:6, seal, heating in water bath in fume hood, and bath temperature is 100 DEG C, reaction
Time is 4h, obtains polyethylene/graphene.
B. the preparation of polyethylene cloth base material/three-layer laminated Graphene/polypyrrole nano line conducing composite material
90.16g potassium peroxydisulfate and 21.2g nitric acid are dissolved in 500mL deionized water to uniform mixed liquor, taking 100mL should
Iron salt mixed liquor, puts into refrigerator lower floor freezing 5min.
By 2.5 × 2.5cm in above-mentioned steps a2Polyethylene cloth base material/Graphene is placed in 2g pyrroles and with 100mL concentration is
In the mixed liquor of the anthraquinone-2-sulfonic acid sodium water solution of 20mg/mL, shaking table mixes 2min, takes out, put into refrigerator lower floor freezing
Taking out after 5min, be together placed in agitator, mixing speed is to be slowly added dropwise the above-mentioned ferrum of 100mL under 600r/min, condition of ice bath
Salt mixed liquor.Take out after reaction 4h and obtain polyethylene cloth base material/three-layer laminated Graphene/polypyrrole nano line conduction composite wood
Material.
Embodiment 11
The present embodiment, with nylon 6 doubling base material as template, is combined one layer of three-layer laminated graphene film on nylon 6,
Nylon 6 doublings/Graphene/polypyrrole nano line flexible conductive composite material is generated under three-layer laminated Graphene inducing action.Institute
State preparation method to follow the steps below:
Prepared by a. nylon 6 doubling/three-layer laminated Graphene
It is 0.3% three-layer laminated graphene oxide that 30cm nylon 6 doubling base material is soaked in concentration, and soak time is 1h,
Obtain nylon 6 doublings/graphene oxide.
Nylon 6 doublings/graphene oxide sample is hung in reactor, adds 10mL ammonia, seal, water in fume hood
Bath heating, bath temperature is 60 DEG C, and the response time is 1h, obtains nylon 6 doublings/Graphene.
The preparation of b. nylon 6 doubling/three-layer laminated Graphene/polypyrrole nano line conducing composite material
127.105g Fe(NO3)39H2O and 6.5g phosphoric acid are dissolved in 500mL deionized water to uniform mixed liquor, take
This iron salt mixed liquor of 100mL, puts into refrigerator lower floor freezing 5min.
30cm nylon 6 doublings/Graphene in above-mentioned steps a being placed in 0.3g pyrroles with 100mL concentration is 5mg/mL's
In the mixed liquor of sodium dodecyl sulfate aqueous solution, shaking table mixes 2min, takes out, take after putting into refrigerator lower floor freezing 5min
Going out, be together placed in agitator, mixing speed is to be slowly added dropwise 100mL above-mentioned iron salt mixed liquor under 600r/min, condition of ice bath.
Take out after reaction 1h and obtain nylon 6 doubling/three-layer laminated Graphene/polypyrrole nano line conducing composite material.
Claims (8)
1. a Graphene inductive formation polypyrrole nano line conducing composite material preparation method, improves Hammers including using
Method prepares three-layer laminated graphene oxide solution, it is characterised in that described preparation method sequentially includes the following steps:
A. prepared by flexible parent metal/three-layer laminated Graphene
Fully being soaked in flexible parent metal to use improves in three-layer laminated graphene oxide solution prepared by Hammers method, three-dimensional
Layered graphite oxide alkene concentration is 0.2%-5%, and flexible parent metal and three-layer laminated graphene oxide soak time are 1-10h, will
Flexible parent metal after immersion hangs in reactor, and adding volume is the reducing agent of 5-30ml, seals, and in fume hood, water-bath adds
Heat, bath temperature is 60-100 DEG C, and the thermal response time is 1-4h, and oxygen-containing group is removed in fully reduction, obtain three-layer laminated Graphene/
Flexible parent metal；
B. the preparation of flexible parent metal/three-layer laminated Graphene/polypyrrole nano line conducing composite material
Three-layer laminated Graphene/flexible parent metal step a obtained is mixed homogeneously on shaking table with pyrroles and surfactant, its
Middle pyrroles and surfactant qualities, than for 1:0.5-2, are together placed in agitator, and mixing speed is 600r/min, at ice bath
Under the conditions of be slowly added to the mixed solution of oxidant and adulterant, wherein oxidant is 1:0.2-2 with the mol ratio of adulterant；Instead
Answer 1-5h, obtain three-layer laminated Graphene/polypyrrole nano line flexible conductive composite material.
A kind of Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation side the most according to claim 1
Method, it is characterised in that: described flexible parent metal be in line base material or cloth base material any one.
A kind of Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation side the most according to claim 2
Method, it is characterised in that: described line base material is the one in nylon 6 doubling or polyethylene strand or cotton thread, and line length substrate is
20-100cm。
A kind of Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation side the most according to claim 2
Method, it is characterised in that: described cloth base material be in carbon cloth or cotton or woven dacron or nylon cloth or polyethylene cloth any one；Cloth
Substrate sizes is 2 × 2-5 × 5cm2。
A kind of Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation side the most according to claim 1
Method, it is characterised in that: described reducing agent is the mixture of ammonia or hydrazine hydrate or hydroiodic acid and glacial acetic acid, the wherein volume of ammonia
Mark is 50%, and the volume fraction of hydrazine hydrate is 85%, and between hydroiodic acid and glacial acetic acid, volume ratio is 1-10:10-1.
A kind of Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation side the most according to claim 1
Method, it is characterised in that: described surfactant is dodecyl sodium sulfate or dodecylbenzene sodium sulfonate or anthraquinone-2-sulfonic acid
In sodium or polyvinylpyrrolidone any one；Described surfactant water concentration is 5-30mg/mL.
A kind of Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation side the most according to claim 1
Method, it is characterised in that: described oxidant is Fe(NO3)39H2O or iron chloride or Ammonium persulfate. or potassium peroxydisulfate or titanium dioxide
In manganese any one.
A kind of Graphene inductive formation polypyrrole nano line flexible conductive composite material preparation side the most according to claim 1
Method, it is characterised in that: described adulterant is appointing in two hydration 5-sulphosalicylic acids or sulphuric acid or hydrochloric acid or phosphoric acid or nitric acid
Meaning one.
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